反应详情

温度

0 °C

Ethyl 6-({3-(aminocarbonyl)-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-thienyl}amino)imidazo[1,2-b]pyridazine-2-carboxylate (33 mg, 0.07 mmol) was taken up in tetrahydrofuran and cooled to 0° C. Trimethylaluminum (0.53 ml, 1.06 mmol) was added dropwise, followed by 3-hydroxyazetidine hydrochloride (7 mg, 0.07 mmol). The reaction was stirred at 0° C. for one hour, warmed to room temperature and allowed to react overnight. The reaction was then quenched slowly with methanol, followed by stirring for 10 minutes at room temperature. The resulting mixture was filtered, washing the solids with ethyl acetate and water. The filtrate was collected, the phases were separated and the aqueous layer was extracted with ethyl acetate. The combined organics were concentrated under and purified via flash chromatography (0-15% methanol in dichloromethane) to afford the title compound.

1. temperaturewarmed to room temperature
2. customto react overnight
3. customThe reaction was then quenched slowly with methanol
4. stirringby stirring for 10 minutes at room temperature
5. filtrationThe resulting mixture was filtered
6. washwashing the solids with ethyl acetate and water
7. customThe filtrate was collected
8. customthe phases were separated
9. extractionthe aqueous layer was extracted with ethyl acetate
10. concentrationThe combined organics were concentrated under and
11. custompurified via flash chromatography (0-15% methanol in dichloromethane)